US10886532B2 - Nanorod-shaped cathode active material for lithium secondary battery, manufacturing method thereof, and lithium secondary battery including the same - Google Patents
Nanorod-shaped cathode active material for lithium secondary battery, manufacturing method thereof, and lithium secondary battery including the same Download PDFInfo
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- US10886532B2 US10886532B2 US16/182,738 US201816182738A US10886532B2 US 10886532 B2 US10886532 B2 US 10886532B2 US 201816182738 A US201816182738 A US 201816182738A US 10886532 B2 US10886532 B2 US 10886532B2
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- United States
- Prior art keywords
- active material
- secondary battery
- lithium secondary
- cathode active
- lithium
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- 239000006182 cathode active material Substances 0.000 title claims abstract description 59
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 56
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 239000002073 nanorod Substances 0.000 claims abstract description 15
- 229910017220 MnxMy Inorganic materials 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims description 19
- 239000002105 nanoparticle Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- -1 nickel metal oxide Chemical class 0.000 claims description 11
- 239000003792 electrolyte Substances 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 239000003002 pH adjusting agent Substances 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 229910044991 metal oxide Inorganic materials 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000006183 anode active material Substances 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 229910021450 lithium metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 229910001416 lithium ion Inorganic materials 0.000 description 8
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical class [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 8
- 239000011572 manganese Substances 0.000 description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 6
- 229910052748 manganese Inorganic materials 0.000 description 6
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- 229910003005 LiNiO2 Inorganic materials 0.000 description 2
- 229910001290 LiPF6 Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 2
- 239000011244 liquid electrolyte Substances 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 229910001537 lithium tetrachloroaluminate Inorganic materials 0.000 description 2
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- ISPYRSDWRDQNSW-UHFFFAOYSA-L manganese(II) sulfate monohydrate Chemical compound O.[Mn+2].[O-]S([O-])(=O)=O ISPYRSDWRDQNSW-UHFFFAOYSA-L 0.000 description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 2
- 239000005518 polymer electrolyte Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- PYOKUURKVVELLB-UHFFFAOYSA-N trimethyl orthoformate Chemical compound COC(OC)OC PYOKUURKVVELLB-UHFFFAOYSA-N 0.000 description 2
- ZZXUZKXVROWEIF-UHFFFAOYSA-N 1,2-butylene carbonate Chemical compound CCC1COC(=O)O1 ZZXUZKXVROWEIF-UHFFFAOYSA-N 0.000 description 1
- CYSGHNMQYZDMIA-UHFFFAOYSA-N 1,3-Dimethyl-2-imidazolidinon Chemical compound CN1CCN(C)C1=O CYSGHNMQYZDMIA-UHFFFAOYSA-N 0.000 description 1
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 description 1
- PPDFQRAASCRJAH-UHFFFAOYSA-N 2-methylthiolane 1,1-dioxide Chemical compound CC1CCCS1(=O)=O PPDFQRAASCRJAH-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 229910001559 LiC4F9SO3 Inorganic materials 0.000 description 1
- 229910014063 LiNi1-xCoxO2 Inorganic materials 0.000 description 1
- 229910014402 LiNi1—xCoxO2 Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical class C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- KLARSDUHONHPRF-UHFFFAOYSA-N [Li].[Mn] Chemical compound [Li].[Mn] KLARSDUHONHPRF-UHFFFAOYSA-N 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 150000004862 dioxolanes Chemical class 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011357 graphitized carbon fiber Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910003480 inorganic solid Inorganic materials 0.000 description 1
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 description 1
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 1
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Chemical compound [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 description 1
- QWGCQZJUWQYRGZ-UHFFFAOYSA-M lithium;difluoromethanesulfonate Chemical compound [Li+].[O-]S(=O)(=O)C(F)F QWGCQZJUWQYRGZ-UHFFFAOYSA-M 0.000 description 1
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- MPDOUGUGIVBSGZ-UHFFFAOYSA-N n-(cyclobutylmethyl)-3-(trifluoromethyl)aniline Chemical compound FC(F)(F)C1=CC=CC(NCC2CCC2)=C1 MPDOUGUGIVBSGZ-UHFFFAOYSA-N 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- AIBQNUOBCRIENU-UHFFFAOYSA-N nickel;dihydrate Chemical compound O.O.[Ni] AIBQNUOBCRIENU-UHFFFAOYSA-N 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- RWRDLPDLKQPQOW-UHFFFAOYSA-N tetrahydropyrrole Substances C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
- C01G51/44—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese
- C01G51/50—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese of the type [MnO2]n-, e.g. Li(CoxMn1-x)O2, Li(MyCoxMn1-x-y)O2
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Definitions
- the present disclosure relates to a nanorod-shaped cathode active material for lithium secondary battery and more particularly, to a cathode active material for lithium secondary battery which has structural stability by controlling the metal composition and particle shape of the cathode active material for lithium secondary battery, a manufacturing method thereof, and a lithium secondary battery including the same.
- lithium secondary batteries having high energy density, high voltage, excellent cycle characteristics and low self-discharge rate have been commercialized and are being widely used.
- Lithium secondary batteries in related arts mainly employ a lithium cobalt composite oxide (LiCoO 2 ) as a main component of a cathode active material.
- the lithium cobalt composite oxide has low stability and is very expensive, and, thus, it has been difficult to mass-produce lithium secondary batteries. Accordingly, the use of a lithium manganese composite oxide, a lithium nickel composite oxide, etc. as an alternative material to the lithium cobalt composite oxide has been considered.
- the lithium nickel composite oxide is cheaper than the lithium cobalt composite oxide and has a reversible capacity close to 200 mAh/g when charged to 4.25 V. Therefore, it is easier to implement large-capacity batteries with the lithium nickel composite oxide than with the lithium cobalt composite oxide having a reversible capacity of 137 mAh/g.
- LiNiO 2 has not been commercialized as a cathode active material in spite of its higher capacity than LiCoO 2 because some Ni ions located in a lithium-ion layer of nonstoichiometric Li 1 ⁇ y Ni 1+y O 2 obstruct the diffusion of lithium ions, which causes a decrease in capacity, and when the amount of lithium is decreased by charge, the oxide is decomposed due to structural instability, and, thus, an oxygen partial pressure is increased and the risk of a battery explosion is increased due to chemical reaction with an organic electrolyte.
- lithium nickel composite oxides represented by LiNi 1 ⁇ x Co x O 2 or LiNi 1 ⁇ x ⁇ y M x M′ y O 2 by substituting a part of nickel with other transition metals such as Co, Mn, etc. to improve structural characteristics of LiNiO 2 -based cathode active materials. If other M 3+ ions with a stable oxidation number are added, it becomes difficult for Ni 2+ to substitute for lithium ions in order to maintain charge neutrality, and, thus, a crystal structure becomes stabilized.
- Article “Trends of development of cathode active material for a lithium secondary battery” in Ceramist Vol. 13, No. 5, October 2010, pp. 32-38 discloses a lithium transition metal oxide, in which a part of nickel is substituted with other transition metals such as manganese, cobalt, etc., as an alternative material.
- a metal-substituted lithium nickel oxide is relatively excellent in cycle characteristics and capacity characteristics, but the cycle characteristics are sharply degraded in case of long-term use and swelling caused by gas generated from a battery and a decrease in thermal safety/stability caused by low chemical stability, which cannot be solved sufficiently.
- An object to be achieved by the present disclosure is to provide a cathode active material for a lithium secondary battery with improved structural stability.
- Another object to be achieved by the present disclosure is to provide a manufacturing method of a cathode active material for a lithium secondary battery which has high structural stability by controlling the metal composition and particle shape of a lithium nickel oxide doped with manganese, magnesium, and mixed metals thereof.
- Yet another object to be achieved by the present disclosure is to provide a lithium secondary battery with improved capacity and lifespan.
- a cathode active material for a lithium secondary battery which is represented by general formula (1) below and has a nanorod shape.
- M is at least one metal selected from the group consisting of Co, Mg, Al, and Cr, 0.5 ⁇ x ⁇ 0.9, and 0 ⁇ y ⁇ 0.1.
- an aspect ratio of the nanorod is in the range of from 5 to 15.
- a manufacturing method of a nanorod-shaped cathode active material for a lithium secondary battery including: preparing a first metal-mixed solution by mixing a nickel metal oxide, a metal oxide, and a solvent; forming first nanoparticles of the first metal-mixed solution; preparing a second metal-mixed solution by mixing the first nanoparticles formed as described above, a lithium metal oxide, and a solvent; and forming second nanoparticles by performing a heat treatment to the second metal-mixed solution, and the forming of the first nanoparticles may be performed by a hydrothermal synthesis.
- the heat treatment is performed in the range of from 400° C. to 800° C.
- the manufacturing method may further include adding a pH adjuster to the first metal-mixed solution.
- the pH adjuster may include an aqueous solution selected from the group consisting of a citric acid aqueous solution, an acrylic acid aqueous solution, an ammonia aqueous solution, and a sodium hydroxide aqueous solution.
- a lithium secondary battery including a nanorod-shaped cathode active material for lithium secondary battery, including: the cathode active material; an anode active material; and an electrolyte.
- a nanorod-shaped cathode active material for lithium secondary battery has a relatively high surface-to-volume ratio and thus can suppress deformation caused by structural deformation of the cathode active material caused during charges and discharges and maximize the lifespan stability.
- a nanorod-shaped cathode active material for lithium secondary battery manufactured by a manufacturing method of a cathode active material for lithium secondary battery according to the present disclosure has a larger contact area with an electrolyte as compared to a nanoparticle or a bulk-type material since the composition and shape of a lithium nickel oxide are controlled by doping a metal such as manganese, magnesium, etc. Therefore, lithium ions have a short migration distance, and, thus, a high charge and discharge capacity can be obtained.
- a lithium secondary battery according to the present disclosure has a large surface area and a high crystallinity, and, thus, the stability can be improved and the capacity retention depending on the speed and number of charges and discharges can be improved.
- FIG. 1( a ) is an SEM image of a nanorod-shaped cathode active material for a lithium secondary battery manufactured according to Example 1;
- FIG. 1( b ) is an SEM image of a nanorod-shaped cathode active material for a lithium secondary battery manufactured according to Comparative Example 1;
- FIG. 1( c ) is an SEM image of a nanorod-shaped cathode active material for a lithium secondary battery manufactured according to Comparative Example 2;
- FIG. 2( a ) is an X-ray diffraction graph before a heat treatment
- FIG. 2( b ) is an X-ray diffraction graph after a heat treatment
- FIG. 3( a ) provides graphs showing a capacity depending on the charge or discharge of a battery.
- FIG. 3( b ) provides graphs showing a capacity depending on the charge or discharge of a battery.
- FIG. 3( c ) provides graphs showing a capacity depending on the charge or discharge of a battery.
- a cathode active material for a lithium secondary battery according to the present disclosure is represented by general formula 1 below and has a nanorod shape. LiNi 1 ⁇ x ⁇ y Mn x M y O 2 (1)
- M is at least one metal selected from the group consisting of Co, Mg, Al, and Cr, 0.5 ⁇ x ⁇ 0.9, and 0 ⁇ y ⁇ 0.1.
- the nanorod-shaped cathode active material for a lithium secondary battery has a larger contact area with an electrolyte as compared to an existing spherical nanoparticle or bulk-type particle.
- lithium ions have a short diffusion distance and a high diffusion rate. Therefore, the nanorod-shaped cathode active material for a lithium secondary battery has a large charge and discharge capacity and exhibits excellent high-speed charge and discharge characteristics.
- the nanorod-shaped cathode active material for a lithium secondary battery has a relatively high surface area-to-volume ratio and thus can suppress structural deformation of the cathode active material caused by consecutive charges and discharges. Therefore, even if the number of charge and discharge cycles is increased, the nanorod-shaped cathode active material for a lithium secondary battery has a high capacity stability.
- an increase in the amount of metal which does not react with lithium may cause a decrease in capacity of the cathode active material.
- the ion radius of a metal is similar to the radius of a lithium ion, different metal may be located at the site of lithium and thus may obstruct the diffusion of lithium.
- an aspect ratio of the nanorod is in the range of from 5 to 15.
- the aspect ratio of the nanorod is less than 5, a contact resistance between electrode active materials may be increased and the electrical conductivity may be decreased, which is not suitable to suppress structural deformation of the cathode active material caused during charges and discharges. If the aspect ratio of the nanorod is more than 15, the diffusion distance of lithium ions is increased, and, thus, capacity characteristics and high-speed charge and discharge characteristics may be degraded.
- the nanorod may have an average thickness in the range of from 15 nm to 30 nm and an average length in the range of from 120 nm to 300 nm.
- a manufacturing method of a nanorod-shaped cathode active material for a lithium secondary battery includes: preparing a first metal-mixed solution by mixing a nickel metal oxide, a metal oxide, and a solvent; forming first nanoparticles of the first metal-mixed solution; preparing a second metal-mixed solution by mixing the first nanoparticles formed as described above, a lithium metal oxide, and a solvent; and forming second nanoparticles by performing a heat treatment to the second metal-mixed solution, and the forming of the first nanoparticles may be performed by a hydrothermal synthesis.
- the heat treatment is performed preferably in the range of from 400° C. to 800° C. and more preferably at 550° C.
- the nanorod may be transformed into a nanoparticle due to flocculation caused by an excessive heat energy. If the heat treatment is performed at less than 400° C., a nanorod-shaped cathode active material having a low crystallinity may be produced.
- the heat treatment may be performed under oxygen atmosphere for 1 to 12 hours.
- the diffusion reaction between metal particles in the metal-mixed solution can be carried out sufficiently and particularly, the reduction of Ni 3+ to Ni 2 ⁇ by carbon dioxide in the air can be suppressed.
- the manufacturing method may further include adding a pH adjuster to the first metal-mixed solution.
- the pH adjuster functions as a precipitant and can maintain a pH suitable for one-dimensional co-precipitation in the first metal-mixed solution.
- the pH adjuster may adjust reaction molar amounts of the co-precipitated elements in the first metal-mixed solution to make a change in particle shape and particle diameter of each of nanoplate, nanowire, nanobelt, etc.
- the pH adjuster may include at least one aqueous solution selected from the group consisting of a citric acid aqueous solution, an acrylic acid aqueous solution, an ammonia aqueous solution, and a sodium hydroxide aqueous solution and may use preferably sodium hydroxide, but is not limited thereto.
- a lithium secondary battery according to the present disclosure may include the cathode active material, an anode active material, and an electrolyte.
- the lithium secondary battery may include a cathode composed of a cathode active material and a current collector, an anode composed of an anode active material and a current collector, and an electrolyte for conduction of lithium ions between the cathode and the anode.
- the anode active material may include one or more members selected from the group consisting of carbonaceous materials such as synthetic graphite, natural graphite, graphitized carbon fibers, amorphous carbon, etc., metallic compounds which can be alloyed with lithium such as silicon (Si), aluminum (Al), tin (Sn), lead (Pb), zinc (Zn), bismuth (Bi), indium (In), manganese (Mn), gallium (Ga), cadmium (Cd), silicon alloys, tin alloys, or aluminum alloys, and composites including the metallic compounds and the carbonaceous materials, but is not limited thereto.
- carbonaceous materials such as synthetic graphite, natural graphite, graphitized carbon fibers, amorphous carbon, etc.
- metallic compounds which can be alloyed with lithium such as silicon (Si), aluminum (Al), tin (Sn), lead (Pb), zinc (Zn), bismuth (Bi), indium (In), manganese (Mn), gallium
- the electrolyte may include one or more members selected from the group consisting of organic liquid electrolytes, inorganic liquid electrolytes, solid-type polymer electrolytes, gel-type polymer electrolytes, inorganic solid electrolytes, and molten-type inorganic electrolytes, but is not limited thereto.
- the electrolyte may include an organic solvent and a lithium salt.
- the organic solvent may include one or more organic solvents selected from the group consisting of N-methyl-2-pyrrolidinone, propylene carbonate, ethylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate, ⁇ -butyrolactone, 1,2-dimethoxyethane, tetrahydroxy Franc, 2-methyltetrahydrofuran, dimethyl sulfoxide, 1,3-dioxolane, formamide, dimethylformamide, dioxolane, acetonitrile, nitromethane, methyl formate, methyl acetate, phosphoric acid triesters, trimethoxymethane, dioxolane derivatives, sulfolane, methylsulfolane, 1,3-dimethyl-2-imidazolidinone, propylene carbonate derivatives, tetrahydrofuran derivatives, ethers, methyl propionate, and ethyl propionate, but is not limited thereto.
- the lithium salt may include one or more members selected from the group consisting of lithium hexafluorophosphate (LiPF 6 ), lithium tetrafluoroborate (LiBF 4 ), lithium hexafluoroantimonate (LiSbF 6 ), lithium hexafluoroarsenate (LiAsF 6 ), lithium difluoromethanesulfonate (LiC 4 F 9 SO 3 ), lithium perchlorate (LiClO 4 ), lithium aluminate (LiAlO 2 ), lithium tetrachloroaluminate (LiAlCl 4 ), lithium chloride (LiCl), lithium iodide (LiI), lithium bis(oxalato)borate (LiB(C 2 O 4 ) 2 ), and lithium trifluoromethanesulfonyl imide, but is not limited thereto.
- LiPF 6 lithium hexafluorophosphate
- LiBF 4 lithium
- NiSO 4 .6H 2 O (Aldrich, 2.06 g), MnSO 4 .H 2 O (Aldrich, 0.12 g), and MgSO 4 (Aldrich, 0.12 g) were dissolved in 40 ml of distilled water and NaOH (Aldrich, 0.02 g) was added to the mixture, which was then reacted at 120° C. for 24 hours by a hydrothermal synthesis to form nanoparticles. Then, LiOH.H 2 O was mixed therein and heat-treated at 550° C. for 12 hours under an oxygen atmosphere to manufacture a nanorod-shaped cathode active material for a lithium secondary battery.
- the cathode active material for a lithium secondary battery has a nanorod shape having an aspect ratio of about 6 as illustrated in FIG. 1A .
- a cathode active material was manufactured in the same manner as described in Example 1 except MgSO 4 (Aldrich, 0.12 g).
- the cathode active material for a lithium secondary battery has a nanorod shape having an aspect ratio of about 4 as illustrated in FIG. 1B .
- An active material was manufactured in the same manner as described in Example 1 except MnSO 4 .H 2 O (Aldrich, 0.12 g) and MgSO 4 (Aldrich, 0.12 g).
- the cathode active material for a lithium secondary battery has a nanorod shape having an aspect ratio of about 17 as illustrated in FIG. 1C .
- Batteries were fabricated by the following method in order to evaluate electrochemical characteristics of secondary batteries including the cathode active materials prepared in Example 1 and Comparative Examples 1 and 2, respectively.
- a 70 wt % cathode active material, 20 wt % conductive carbon black, and a 10 wt % polyvinylidene fluoride binder were mixed with NMP (N-methyl-2-pyrrolidine) to prepare slurry.
- NMP N-methyl-2-pyrrolidine
- the slurry was applied to aluminum foil and then dried and rolled to prepare a cathode.
- the cathode, lithium metal, and a separator were used to fabricate a coin cell.
- a solution including 1.0 M LiPF 6 dissolved in a 1:1-mixed solution of ethylene carbonate (EC) and diethyl carbonate (DEC) was used as an electrolyte.
- a diffraction pattern 10 , a diffraction pattern 20 , and a diffraction pattern 30 represent X-ray diffraction graphs for a Mn and Mg-doped nickel hydroxide, a Mn-doped nickel hydroxide, and a nickel hydroxide nanowire precursor, respectively.
- a diffraction pattern 40 in FIG. 2B represents an X-ray diffraction graph for a Mn and Mg-doped lithium nickel oxide cathode active material prepared according to Example 1, a diffraction pattern 50 in FIG.
- FIG. 2B represents an X-ray diffraction graph for a Mn-doped lithium nickel oxide cathode active material prepared according to Comparative Example 1, and a diffraction pattern 60 in FIG. 2B represents an X-ray diffraction graph for a lithium nickel oxide cathode active material prepared according to Comparative Example 2.
- the diffraction pattern 10 , the diffraction pattern 20 , and the diffraction pattern 30 for precursor nanowire in FIG. 2A show that the diffraction lines move to lower angles depending on doping, which means that the lattice constants increase with doping.
- the diffraction pattern 40 , the diffraction pattern 50 , and the diffraction pattern 60 after a high-temperature solid-state reaction in FIG. 2B show the absence of other impurities and excellent crystallinity. Particularly, it can be seen that a diffraction line 70 of the diffraction pattern 40 for the Mn and Mg-doped lithium nickel oxide has the most significant phase and the crystallinity increases.
- a battery including the cathode active material prepared in Example 1 as illustrated in FIG. 3A has an initial discharge capacity of 90.0 mAh/g and a discharge capacity equivalent to 69% or more of the initial discharge capacity after 15 charge and discharge cycles.
- a battery including the cathode active material prepared in Comparative Example 1 as illustrated in FIG. 3B has an initial discharge capacity of 84.6 mAh/g and a discharge capacity equivalent to less than 62% of the initial discharge capacity after 15 charge and discharge cycles.
- a battery including the cathode active material prepared in Comparative Example 2 as illustrated in FIG. 3C has an initial discharge capacity of 68.2 mAh/g and a discharge capacity equivalent to less than 75% of the initial discharge capacity after 15 charge and discharge cycles.
- the Mn and Mg-doped lithium nickel oxide cathode active material shows a slight decrease in initial stability but also shows an increase in charge and discharge capacity.
- the battery including the cathode active material prepared in Example 1 has the highest initial discharge capacity and a considerable discharge capacity retention and thus shows the highest discharge capacity even after 15 charge and discharge cycles.
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Abstract
LiNi1−x−yMnxMyO2 (1)
Description
LiNi1−x−yMnxMyO2 (1)
LiNi1−x−yMnxMyO2 (1)
Claims (7)
LiNi1−x−yMnxMyO2 (1)
LiNi1−x−yMnxMyO2 (1)
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KR20100107788A (en) | 2009-03-26 | 2010-10-06 | 한국과학기술원 | Method for preparing lithium manganese oxide and lithium manganese metal oxide with spinel and nanostructure |
CN103296270A (en) * | 2013-06-14 | 2013-09-11 | 江苏海四达电源股份有限公司 | Lithium-ion battery positive material lithium nickel manganese cobalt (LiNixCoyMnzO2) and preparation method thereof |
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CN103296270A (en) * | 2013-06-14 | 2013-09-11 | 江苏海四达电源股份有限公司 | Lithium-ion battery positive material lithium nickel manganese cobalt (LiNixCoyMnzO2) and preparation method thereof |
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Trends of development of cathode active material for a lithium secondary battery in Ceramist vol. 13, No. 5, Oct. 2010, pp. 32-38. |
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